CN106219483A - A kind of preparation method of microelectrode array - Google Patents
A kind of preparation method of microelectrode array Download PDFInfo
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- CN106219483A CN106219483A CN201610647207.7A CN201610647207A CN106219483A CN 106219483 A CN106219483 A CN 106219483A CN 201610647207 A CN201610647207 A CN 201610647207A CN 106219483 A CN106219483 A CN 106219483A
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- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00214—Processes for the simultaneaous manufacturing of a network or an array of similar microstructural devices
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Abstract
The present invention relates to photosensitive gel technique field, particularly to the preparation method of a kind of microelectrode array.Comprise the following steps: step 1: by tetraethyl orthosilicate and dehydrated alcohol mix and blend 20 40min, add 1,10 luxuriant and rich with fragrance quinolines, deionized water and hydrochloric acid, continue stirring 2 3h, be aged 24 48h, obtain the photosensitive colloidal sol of silicon dioxide；The mol ratio of above-mentioned interpolation reagent is tetraethyl orthosilicate: dehydrated alcohol: 1,10 luxuriant and rich with fragrance quinolines: deionized water: hydrochloric acid=5:100 200:2.5:10:1；Step 2: the photosensitive colloidal sol of silicon dioxide using step 1 to prepare prepares silicon dioxide photosensitive film at substrate；Mask plate is placed in described silicon dioxide photosensitive film surface, exposes 30 60min under ultraviolet light, after dehydrated alcohol dissolves and washes away development, obtain microelectrode array.
Description
Technical field
The present invention relates to photosensitive gel technique field, particularly to the preparation method of a kind of microelectrode array.
Background technology
Microelectrode array has that size is little, integrated level is high, has the highest mass transfer rate and electrode signal to noise ratio, accordingly speed
Degree is fast, sensitivity advantages of higher, is widely used in fields such as electrochemistry, sensor, microelectronics.
Traditional film microelectrode arrays is mainly by means of the photoetching technique in MEMS.The method utilizes the light of light-sensitive medium
-chemical principle forms active graphical, and later stage auxiliary etch means obtain Target Aerial Array；Have an advantage in that: technology maturation,
It is easy to large area, extensive quick acquisition array pattern and resolution higher, is disadvantageous in that in photoetching technique and mostly uses
Conventional lithography glue is as light-sensitive medium.
At present, the photoresist that steady quality, resolution are high the most all needs import, and this is just for preparation large area microarray electricity
Pole adds production cost and technical limitations.And use the synthesis of photosensitive sol-gel process to have the photosensitive silicon dioxide of ultraviolet
Colloidal sol and gel film thereof, the research being applied to film microelectrode arrays have not been reported.
Summary of the invention
The technical problem to be solved is: provide the preparation method of a kind of microelectrode array, solves traditional micro-electricity
Array used import photoresist in pole is as light-sensitive medium, the problem bringing high cost when preparing large area tiny array electrode.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is: provide the preparation of a kind of microelectrode array
Method, comprises the following steps:
Step 1: by tetraethyl orthosilicate and dehydrated alcohol mix and blend 20-40min, adds 1,10-phenanthrene quinoline, deionized water
And hydrochloric acid, continue stirring 2-3h, be aged 24-48h, obtain the photosensitive colloidal sol of silicon dioxide；The mol ratio of above-mentioned interpolation reagent is just
Silester: dehydrated alcohol: 1,10-phenanthrene quinoline: deionized water: hydrochloric acid=5:100-200:2.5:10:1；
Step 2: the photosensitive colloidal sol of silicon dioxide using step 1 to prepare prepares silicon dioxide photosensitive film at substrate；To cover
Film version is placed in described silicon dioxide photosensitive film surface, exposes 30-60min under ultraviolet light, after dehydrated alcohol dissolves and washes away development
Obtain microelectrode array.
The beneficial effects of the present invention is: use silicon dioxide gel and gel technique thereof to combine ultraviolet mask irradiation method and exist
Microelectrode array is prepared on substrate；The place that silica membrane covers substrate is non-conductive, and the part exposing substrate has good
Good electric conductivity；Microelectrode array preparation manipulation simplicity, low cost that the present invention provides, efficiency is fast, quality is high, is suitable for preparation greatly
Area microelectrode array.
Accompanying drawing explanation
Fig. 1 is the ultraviolet spectra that silicon dioxide photosensitive film changes with ultraviolet lighting；
Fig. 2-a to Fig. 2-d is the microelectrode array in monocrystalline substrate；
Fig. 3-a to Fig. 3-b is the microelectrode array in FTO glass substrate；
Fig. 4-a to Fig. 4-b is the microelectrode array in ITO flexible substrate.
Detailed description of the invention
By describing the technology contents of the present invention in detail, being realized purpose and effect, it is explained below in conjunction with embodiment.
The design of most critical of the present invention is: use silicon dioxide gel and gel technique thereof to combine ultraviolet mask irradiation method
Substrate is prepared microelectrode array；Preparation manipulation simplicity, low cost, efficiency is fast, quality is high, is suitable for preparation large area microelectrode
Array.
The present invention provides the preparation method of a kind of microelectrode array, comprises the following steps:
Step 1: the preparation of the photosensitive colloidal sol of silicon dioxide: by tetraethyl orthosilicate and dehydrated alcohol mix and blend 20-40min,
Adding 1,10-phenanthrene quinoline, deionized water and hydrochloric acid, continuation is stirred 2-3h, is aged 24-48h, obtains the photosensitive colloidal sol of silicon dioxide；
The mol ratio of above-mentioned interpolation reagent is tetraethyl orthosilicate: dehydrated alcohol: 1,10-phenanthrene quinoline: deionized water: hydrochloric acid=5:100-
200:2.5:10:1；
Step 2: the preparation of photosensitive film and graphical: use the photosensitive colloidal sol of silicon dioxide that step 1 prepares at substrate
Prepare silicon dioxide photosensitive film；Mask plate is placed in described silicon dioxide photosensitive film surface, exposes 30-under ultraviolet light
60min, obtains microelectrode array after dehydrated alcohol dissolves and washes away development.
Knowable to foregoing description, the beneficial effects of the present invention is: use silicon dioxide gel and gel technique thereof to combine
Ultraviolet mask irradiation method prepares microelectrode array on substrate；The place that silica membrane covers substrate is non-conductive, and exposes
The part of substrate has good electric conductivity；Microelectrode array preparation manipulation simplicity that the present invention provides, low cost, efficiency soon,
Quality is high, is suitable for preparation large area microelectrode array.
Further, the preparation method of a kind of microelectrode array, the preparation side of the photosensitive colloidal sol of silicon dioxide in described step 1
Method is: by tetraethyl orthosilicate and dehydrated alcohol mix and blend 30min, addition 1,10-phenanthrene quinoline, deionized water and hydrochloric acid, continue
Stirring 3h, is aged 36h, obtains the photosensitive colloidal sol of silicon dioxide；The mol ratio of above-mentioned interpolation reagent is tetraethyl orthosilicate: anhydrous second
Alcohol: 1,10-phenanthrene quinoline: deionized water: hydrochloric acid=5:100-200:2.5:10:1.
Seen from the above description, the compound method of the photosensitive colloidal sol of further preferred silicon dioxide, thus obtain high-quality
The photosensitive colloidal sol of silicon dioxide.
Further, all processes of described step 1 are all carried out in nitrogen glove box.
Owing to microelectrode array is precise structure, high to photosensitive colloidal sol prescription, operate in nitrogen glove box and can have
Effect prevents the composition in air from polluting photosensitive colloidal sol.
Further, the pull rate using dip-coating method in described step 2 is 90-200mm/min.
The preferably pull rate of dip-coating method, ensures the uniformity of photosensitive film while ensureing preparation efficiency.
Further, in described step 2, substrate uses monocrystal silicon, FTO glass or ITO flexible substrate.
Use above-mentioned quasiconductor as the backing material of microelectrode array, there is, uv absorption good to visible light transmission
The advantage that coefficient is big, resistivity is low, antiacid alkali ability is strong under stable chemical performance and room temperature.
Further, described step 2 medium ultraviolet light uses wavelength 365nm, and power is the SP-9 type ultraviolet point light of 250mW
Source.
Seen from the above description, as it is shown in figure 1, have the photosensitive silicon dioxide gel of ultraviolet and the light of gel film thereof
Sensing wavelengths centered lays respectively at 225 and 267nm, and after ultraviolet lighting a period of time, absorption peak strength declines, chela in thin film
Close structure generation photolysis, preferably ultraviolet point source condition, improve difficult to understand in thin film and the photolysis efficiency of structure.
Embodiment 1
Refer to Fig. 2-a to Fig. 2-d, the preparation method of a kind of microelectrode array, comprise the following steps:
Step 1: the preparation of the photosensitive colloidal sol of silicon dioxide: by tetraethyl orthosilicate and dehydrated alcohol mix and blend 30min, adds
1,10-phenanthrene quinoline, deionized water and hydrochloric acid, continue stirring 3h, be aged 36h, obtains silicon dioxide photosensitive colloidal sol above-mentioned interpolation examination
The mol ratio of agent is tetraethyl orthosilicate: dehydrated alcohol: 1,10-phenanthrene quinoline: deionized water: hydrochloric acid=5:100-200:2.5:10:
1；All processes are all carried out in nitrogen glove box；
Step 2: the preparation of photosensitive film and graphical: use the photosensitive colloidal sol of silicon dioxide that step 1 prepares at monocrystalline
Preparing silicon dioxide photosensitive film on silicon substrate, pull rate is 90-200mm/min, and then mask plate is placed in film surface,
Exposing 30-60min under ultraviolet light, ultraviolet light uses wavelength 365nm, and power is the SP-9 type ultraviolet point source of 250mW, through nothing
Water-ethanol obtains microarray figure after dissolveing and washing away development.
Embodiment 2
Refer to Fig. 3-a and Fig. 3-b, the preparation method of a kind of microelectrode array, comprise the following steps:
Step 1: the preparation of the photosensitive colloidal sol of silicon dioxide: by tetraethyl orthosilicate and dehydrated alcohol mix and blend 30min, adds
1,10-phenanthrene quinoline, deionized water and hydrochloric acid, continue stirring 3h, be aged 36h, obtain the photosensitive colloidal sol of silicon dioxide；Above-mentioned interpolation tries
The mol ratio of agent is tetraethyl orthosilicate: dehydrated alcohol: 1,10-phenanthrene quinoline: deionized water: hydrochloric acid=5:100-200:2.5:10:
1；All processes are all carried out in nitrogen glove box；
Step 2: the preparation of photosensitive film and graphical: use the photosensitive colloidal sol of silicon dioxide that step 1 prepares at FTO glass
Preparing silicon dioxide photosensitive film on glass substrate, pull rate is 90-200mm/min, and then mask plate is placed in film surface,
Exposing 30-60min under ultraviolet light, ultraviolet light uses wavelength 365nm, and power is the SP-9 type ultraviolet point source of 250mW, through nothing
Water-ethanol obtains microarray figure after dissolveing and washing away development.
Embodiment 3
Refer to Fig. 4-a and Fig. 4-b, the preparation method of a kind of microelectrode array, comprise the following steps:
Step 1: the preparation of the photosensitive colloidal sol of silicon dioxide: by tetraethyl orthosilicate and dehydrated alcohol mix and blend 30min, adds
1,10-phenanthrene quinoline, deionized water and hydrochloric acid, continue stirring 3h, be aged 36h, obtain the photosensitive colloidal sol of silicon dioxide；Above-mentioned interpolation tries
The mol ratio of agent is tetraethyl orthosilicate: dehydrated alcohol: 1,10-phenanthrene quinoline: deionized water: hydrochloric acid=5:100-200:2.5:10:
1；All processes are all carried out in nitrogen glove box；
Step 2: the preparation of photosensitive film and graphical: the photosensitive colloidal sol of silicon dioxide using step 1 to prepare is soft at ITO
Preparing silicon dioxide photosensitive film on property substrate, pull rate is 90-200mm/min, and then mask plate is placed in film surface,
Exposing 30-60min under ultraviolet light, ultraviolet light uses wavelength 365nm, and power is the SP-9 type ultraviolet point source of 250mW, through nothing
Water-ethanol obtains microarray figure after dissolveing and washing away development.
In sum, the preparation method of the microelectrode array that the present invention provides, have the beneficial effects that: use silicon dioxide molten
Glue and gel technique thereof combine ultraviolet mask irradiation method and prepare microelectrode array on substrate；Silica membrane covers substrate
Local non-conductive, and the part exposing substrate has good electric conductivity；The microelectrode array preparation manipulation letter that the present invention provides
Just, low cost, efficiency are fast, quality is high, are suitable for preparation large area microelectrode array.
The further preferably compound method of the photosensitive colloidal sol of silicon dioxide, thus it is photosensitive molten to obtain high-quality silicon dioxide
Glue；Owing to microelectrode array is precise structure, high to photosensitive colloidal sol prescription, operate in nitrogen glove box and can effectively prevent
Composition in air pollutes photosensitive colloidal sol；The preferably pull rate of dip-coating method, ensures sense while ensureing preparation efficiency
The uniformity of optical thin film；Using above-mentioned quasiconductor as the backing material of microelectrode array, it is good to visible light transmission, purple to have
The advantage that outer absorptance is big, resistivity is low, antiacid alkali ability is strong under stable chemical performance and room temperature；As it is shown in figure 1, have
The photoinduction wavelengths centered of the photosensitive silicon dioxide gel of ultraviolet and gel film thereof lays respectively at 225 and 267nm, along with purple
After outer illumination a period of time, absorption peak strength declines, chelate structure generation photolysis in thin film, preferably ultraviolet point source condition,
Improve difficult to understand in thin film and the photolysis efficiency of structure.
The foregoing is only embodiments of the invention, not thereby limit the scope of the claims of the present invention, every utilize this
The equivalents that bright description is made, or directly or indirectly it is used in relevant technical field, the most in like manner it is included in this
In bright scope of patent protection.
Claims (6)
1. the preparation method of a microelectrode array, it is characterised in that comprise the following steps:
Step 1: by tetraethyl orthosilicate and dehydrated alcohol mix and blend 20-40min, adds 1,10-phenanthrene quinoline, deionized water and salt
Acid, continues stirring 2-3h, is aged 24-48h, obtains the photosensitive colloidal sol of silicon dioxide；The mol ratio of above-mentioned interpolation reagent is positive silicic acid
Ethyl ester: dehydrated alcohol: 1,10-phenanthrene quinoline: deionized water: hydrochloric acid=5:100-200:2.5:10:1；
Step 2: the photosensitive colloidal sol of silicon dioxide using step 1 to prepare prepares silicon dioxide photosensitive film at substrate；By mask plate
It is placed in described silicon dioxide photosensitive film surface, exposes 30-60min under ultraviolet light, obtain after dehydrated alcohol dissolves and washes away development
Microelectrode array.
The preparation method of microelectrode array the most according to claim 1, it is characterised in that: silicon dioxide in described step 1
The compound method of photosensitive colloidal sol is: by tetraethyl orthosilicate and dehydrated alcohol mix and blend 30min, adds 1,10-phenanthrene quinoline, go from
Sub-water and hydrochloric acid, continue stirring 3h, be aged 36h, and the mol ratio of above-mentioned interpolation reagent is tetraethyl orthosilicate: dehydrated alcohol: 1,10-
Luxuriant and rich with fragrance quinoline: deionized water: hydrochloric acid=5:100-200:2.5:10:1.
The preparation method of microelectrode array the most according to claim 1, it is characterised in that: all processes of described step 1
All carry out in nitrogen glove box.
The preparation method of microelectrode array the most according to claim 1, it is characterised in that: described step 2 uses dipping
The pull rate of czochralski method is 90-200mm/min.
The preparation method of microelectrode array the most according to claim 1, it is characterised in that: in described step 2, substrate uses
Monocrystal silicon, FTO glass or ITO flexible substrate.
The preparation method of microelectrode array the most according to claim 1, it is characterised in that: described step 2 medium ultraviolet gloss
Using wavelength 365nm, power is the SP-9 type ultraviolet point source of 250mW.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109319731A (en) * | 2018-10-31 | 2019-02-12 | 福建师范大学 | A kind of preparation method of microelectrode array |
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